PREPARATION METHOD FOR 4-(HYDROXYMETHYLPHOSPHINYL)-2-OXOBUTYRIC ACID

• Main Authors: WANG, Linlin, QIN, Long, WANG, Ping, YANG, Lirong, WU, Jianping, ZHOU, Shuguang, ZHAN, Bo, ZHOU, Haisheng, YU, Shenluan
• Format: Patent
• Language: Chinese; English; French
• Published: 14.03.2024
• Subjects: ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAININGELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN,SULFUR, SELENIUM OR TELLURIUM; CHEMISTRY; METALLURGY; ORGANIC CHEMISTRY

A preparation method for 4-(hydroxymethylphosphinyl)-2-oxobutyric acid, comprising the following steps: a) mixing 3-chloropropionyl chloride, a first solvent, trimethylsilyl cyanide, and a cyanide salt, carrying out a substitution reaction to obtain a feed liquid containing 4-chloro-2-oxobutyronitrile, and then carrying out reduced pressure distillation and separation to obtain a 4-chloro-2-oxobutyronitrile intermediate; b) carrying out Arbuzov reaction on the obtained 4-chloro-2-oxobutyronitrile intermediate and methyl phosphonite in a second solvent in the presence of cuprous iodide to obtain a feed liquid of (3-cyano-3-oxopropyl)methyl phosphinate, and purifying to obtain a crude product of (3-cyano-3-oxopropyl)methyl phosphinate; and c) mixing the obtained crude product of (3-cyano-3-oxopropyl)methyl phosphinate with hydrochloric acid, carrying out a hydrolysis reaction, and then carrying out purification treatment to obtain 4-(hydroxymethylphosphinyl)-2-oxobutyric acid. According to the preparation metho